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  • 1
    ISSN: 1612-1112
    Keywords: Micellar electrokinetic capillary chromatography ; Enkephalin related peptides ; Response surface modelling ; Central composite designs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simultaneous optimization of resolution, efficiency and migration times of enkephalin-related peptides in micellar electrokinetic capillary chromatography (MEKC) was performed. Six experimental variables; the surfactant concentration, the percentage of organic modifier, the ionic strength of the buffer, the injected plug length, the applied temperature and the sample solution composition were studied via central composite design (CCD). Large differences in separation performance were observed at a commonly used level of organic modifier in the background electrolyte. Partial least squares regression of the responses revealed that the experimental domain was too large and complicated to be explained by the model. A new CCD model was obtained with improved prediction ability at narrower ranges of the experimental factors, especially of the organic modifier. A conflict between maximum resolution and efficiency within the shortest analysis time was observed. Therefore, constraints were set on maximal resolution and analysis time, while solving for maximum efficiency. Optimal operating conditions were found at 35 mM sodium dodecyl sulfate (SDS), 5% v/v of acetonitrile, 1.9 mm injected plug length, 35°C and sample solution with no added micelles, giving high efficiency and resolution at short analysis time. The value predicted by the model was found to agree very well to the observed values, at the optimal experimental conditions, even on a new capillary.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; Drug purity ; Frequency doubled laser ; Laser induced fluorescence ; Reduced electromigration dispersion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In drug purity determinations by capillary electrophoresis using UV-detection generally a relative high concentration of the main compound has to be injected. Principles how to handle overloading effects are described. NXX-066 is a drug with a native fluorescence which made it possible to use of CE system equipped with a LIF-detection unit. Monitoring drug purity determination with LIF detection results in an improved limit of quantification of the impurities and/or opens a possibility to avoid an overloaded main peak. A frequency doubled (FRED) argon ion laser set at 244 nm was used as excitation source in drug purity determination with the LIF-detection unit and the chemicals used were therefore carefully chosen in order to minimize the background noise level, which easily is enhanced when fluorescence detection is performed in the UV-range. The separation of the fluorescent NXX-066 analogues proved to be a difficult task, but an adequate resolution was obtained when β- and γ-cyclodextrins was added as structural selectors and the separation window was expanded by the use of a repressed/reversed electroosmotic flow. A comparison of the separation capability for the UV-detection system and the laser induced fluorescence detection system was performed, showing that the overloading effects of the main peak can be removed using the CE-LIF system and thereby obtain a substantially improved resolution of the analogues. A comparison of LC-UV and CE-UV for drug purity determination of a crude product from, synthesis of NXX-066 is also included in this paper where a good correlation of the results were obtained.
    Type of Medium: Electronic Resource
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